#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/57/4305729.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4305729
loop_
_publ_author_name
'Diane A. Kanas'
'Stephen J. Geier'
'Christopher M. Vogels'
'Andreas Decken'
'Stephen A. Westcott'
_publ_contact_author_address
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_fax         '(506) 453-4981'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_phone       '(506) 453-4875'
_publ_section_title
;
Synthesis, Characterization, and Reactivity of Rhodium(I) Acetylacetonato
Complexes Containing Pyridinecarboxaldimine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8727
_journal_page_last               8735
_journal_paper_doi               10.1021/ic800703n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C19 H21 N2 O2 Rh'
_chemical_formula_sum            'C19 H21 N2 O2 Rh'
_chemical_formula_weight         412.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.896(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.442(6)
_cell_length_b                   7.753(5)
_cell_length_c                   24.080(16)
_cell_measurement_reflns_used    6865
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.76
_cell_volume                     1763(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10923
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.9526
_exptl_absorpt_correction_T_min  0.6664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         10923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0643P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                9287
_reflns_number_total             10923
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic800703n_si_001_2.cif
_cod_data_source_block           sw060490
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305729
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh Rh 0.20923(3) 0.35505(4) 0.111687(11) 0.02076(15) Uani 1 1 d . . .
N1 N 0.3585(3) 0.2186(4) 0.07664(11) 0.0223(7) Uani 1 1 d . . .
N2 N 0.1095(3) 0.2834(4) 0.04255(11) 0.0216(7) Uani 1 1 d . . .
O1 O 0.3307(2) 0.4257(3) 0.17711(10) 0.0244(6) Uani 1 1 d . . .
O2 O 0.0396(2) 0.4795(3) 0.14131(9) 0.0244(6) Uani 1 1 d . . .
C1 C 0.3280(4) 0.1535(5) 0.02826(14) 0.0270(8) Uani 1 1 d . . .
H1 H 0.3942 0.0866 0.0082 0.032 Uiso 1 1 calc R . .
C2 C 0.1898(4) 0.1882(4) 0.00708(14) 0.0237(8) Uani 1 1 d . . .
C3 C 0.1341(4) 0.1307(5) -0.04330(14) 0.0315(9) Uani 1 1 d . . .
H3 H 0.1912 0.0648 -0.0675 0.038 Uiso 1 1 calc R . .
C4 C -0.0034(4) 0.1691(5) -0.05821(15) 0.0322(9) Uani 1 1 d . . .
H4 H -0.0426 0.1296 -0.0925 0.039 Uiso 1 1 calc R . .
C5 C -0.0829(4) 0.2657(5) -0.02249(15) 0.0322(9) Uani 1 1 d . . .
H5 H -0.1780 0.2942 -0.0321 0.039 Uiso 1 1 calc R . .
C6 C -0.0256(4) 0.3210(4) 0.02688(15) 0.0270(9) Uani 1 1 d . . .
H6 H -0.0823 0.3880 0.0510 0.032 Uiso 1 1 calc R . .
C7 C 0.4903(3) 0.1712(4) 0.10373(14) 0.0227(8) Uani 1 1 d . . .
C8 C 0.4968(4) 0.0125(5) 0.13107(15) 0.0269(8) Uani 1 1 d . . .
C9 C 0.6208(4) -0.0283(5) 0.15980(15) 0.0305(9) Uani 1 1 d . . .
H9 H 0.6290 -0.1367 0.1780 0.037 Uiso 1 1 calc R . .
C10 C 0.7320(4) 0.0859(5) 0.16228(16) 0.0349(10) Uani 1 1 d . . .
H10 H 0.8153 0.0571 0.1828 0.042 Uiso 1 1 calc R . .
C11 C 0.7233(4) 0.2410(5) 0.13528(15) 0.0320(9) Uani 1 1 d . . .
H11 H 0.8021 0.3171 0.1367 0.038 Uiso 1 1 calc R . .
C12 C 0.6020(4) 0.2898(5) 0.10591(16) 0.0275(9) Uani 1 1 d . . .
C13 C 0.3744(4) -0.1112(5) 0.12989(18) 0.0385(11) Uani 1 1 d . . .
H13A H 0.3708 -0.1706 0.0940 0.058 Uiso 1 1 calc R . .
H13B H 0.2860 -0.0476 0.1352 0.058 Uiso 1 1 calc R . .
H13C H 0.3867 -0.1962 0.1597 0.058 Uiso 1 1 calc R . .
C14 C 0.5915(4) 0.4608(5) 0.07674(18) 0.0422(11) Uani 1 1 d . . .
H14A H 0.6665 0.5375 0.0906 0.063 Uiso 1 1 calc R . .
H14B H 0.4989 0.5127 0.0839 0.063 Uiso 1 1 calc R . .
H14C H 0.6021 0.4437 0.0367 0.063 Uiso 1 1 calc R . .
C15 C 0.2891(4) 0.5203(5) 0.21687(14) 0.0238(8) Uani 1 1 d . . .
C16 C 0.1512(4) 0.5831(5) 0.22358(15) 0.0252(8) Uani 1 1 d . . .
H16 H 0.1341 0.6473 0.2564 0.030 Uiso 1 1 calc R . .
C17 C 0.0381(4) 0.5613(4) 0.18746(14) 0.0231(8) Uani 1 1 d . . .
C18 C 0.4018(4) 0.5637(5) 0.25925(16) 0.0358(10) Uani 1 1 d . . .
H18A H 0.4172 0.4646 0.2839 0.054 Uiso 1 1 calc R . .
H18B H 0.3716 0.6633 0.2811 0.054 Uiso 1 1 calc R . .
H18C H 0.4902 0.5913 0.2404 0.054 Uiso 1 1 calc R . .
C19 C -0.1027(4) 0.6417(5) 0.20063(15) 0.0333(9) Uani 1 1 d . . .
H19A H -0.1314 0.7195 0.1704 0.050 Uiso 1 1 calc R . .
H19B H -0.0943 0.7069 0.2354 0.050 Uiso 1 1 calc R . .
H19C H -0.1740 0.5508 0.2046 0.050 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh N2 79.78(12) . . ?
N1 Rh O1 94.55(11) . . ?
N2 Rh O1 173.60(10) . . ?
N1 Rh O2 172.93(10) . . ?
N2 Rh O2 93.54(11) . . ?
O1 Rh O2 92.24(10) . . ?
C1 N1 C7 119.0(3) . . ?
C1 N1 Rh 116.4(2) . . ?
C7 N1 Rh 124.2(2) . . ?
C6 N2 C2 118.1(3) . . ?
C6 N2 Rh 127.3(2) . . ?
C2 N2 Rh 114.5(2) . . ?
C15 O1 Rh 124.6(2) . . ?
C17 O2 Rh 124.4(2) . . ?
N1 C1 C2 116.0(3) . . ?
N1 C1 H1 122.0 . . ?
C2 C1 H1 122.0 . . ?
N2 C2 C3 120.8(3) . . ?
N2 C2 C1 113.2(3) . . ?
C3 C2 C1 125.9(3) . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 118.5(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
N2 C6 C5 122.1(3) . . ?
N2 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
C8 C7 C12 122.2(3) . . ?
C8 C7 N1 117.9(3) . . ?
C12 C7 N1 119.6(3) . . ?
C9 C8 C7 117.8(3) . . ?
C9 C8 C13 120.5(4) . . ?
C7 C8 C13 121.7(3) . . ?
C10 C9 C8 120.9(4) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 121.6(4) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C7 117.1(4) . . ?
C11 C12 C14 121.8(3) . . ?
C7 C12 C14 121.2(3) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 C15 C16 125.8(3) . . ?
O1 C15 C18 114.7(3) . . ?
C16 C15 C18 119.6(3) . . ?
C17 C16 C15 126.7(3) . . ?
C17 C16 H16 116.7 . . ?
C15 C16 H16 116.7 . . ?
O2 C17 C16 126.2(3) . . ?
O2 C17 C19 114.1(3) . . ?
C16 C17 C19 119.7(3) . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh N1 1.963(3) . ?
Rh N2 1.980(3) . ?
Rh O1 2.010(2) . ?
Rh O2 2.010(2) . ?
N1 C1 1.298(4) . ?
N1 C7 1.444(4) . ?
N2 C6 1.356(4) . ?
N2 C2 1.368(4) . ?
O1 C15 1.273(4) . ?
O2 C17 1.280(4) . ?
C1 C2 1.419(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(5) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.367(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.396(5) . ?
C7 C12 1.400(5) . ?
C8 C9 1.387(5) . ?
C8 C13 1.502(5) . ?
C9 C10 1.374(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9500 . ?
C12 C14 1.503(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.402(5) . ?
C15 C18 1.501(5) . ?
C16 C17 1.377(5) . ?
C16 H16 0.9500 . ?
C17 C19 1.507(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
